ABSTRACT
Simple micellar electrokinetic chromatographic (MEKC) method was developed for the determination of ketoprofen as the active substance and methylparaben and propylparaben as preservatives in a semisolid pharmaceutical preparation. Separation was carried out with a fused silica capillary and UV detection at 200nm. Optimized background electrolyte was 50mM tricine buffer containing 30mM sodium dodecyl sulfate as surfactant and 15% (v/v) of methanol. Single separation took about 13min. No statistically significant differences were found when comparing the results with those of RP-HPLC method reported in literature.
Subject(s)
Chromatography, Micellar Electrokinetic Capillary/methods , Ketoprofen/analysis , Parabens/analysisABSTRACT
A method utilising isotachophoresis and capillary zone electrophoresis in the column coupling configuration with UV detection at 320 nm was developed for separation and determination of five phenolic acids (rosmarinic, p-coumaric, ferulic, caffeic and chlorogenic) and flavonoid quercitrin in a methanolic extract of Melissae herba. The proposed method has been validated with correlation coefficients from 0.9842 to 0.9988, RSD values between 0.39% and 0.83% for migration times and between 0.40% and 2.05% for peak areas.
Subject(s)
Antioxidants/analysis , Electrophoresis, Capillary/instrumentation , Electrophoresis/instrumentation , Melissa/chemistry , Plant Extracts/analysis , Specimen Handling/instrumentation , Antioxidants/chemistry , Electrophoresis/methods , Electrophoresis, Capillary/methods , Flavonoids/analysis , Hydrogen-Ion Concentration , Hydroxybenzoates/analysis , Methanol/chemistry , Reproducibility of Results , Sensitivity and Specificity , Specimen Handling/methods , Spectrophotometry, UltravioletABSTRACT
Capillary zone electrophoresis with indirect UV detection at 215 nm was applied for the separation and determination of mannitol (MA), sorbitol (SO) and xylitol in the form of anionic borate-polyol complexes. The separation was carried out in a fused silica capillary (total length 60 cm, effective length 50 cm, I.D. 50 microm) at 25 kV. The optimized background electrolyte was 200 mM borate buffer (pH 9.3, adjusted with triethylamine) containing 10 mM 3-nitrobenzoate as the chromogenic co-ion. The separation took approximately 13 min. The rectilinear calibration range was 0.2-2 mg mL(-1) for MA and SO when using xylitol (1 mg mL(-1)) as the internal standard. The limit of detection at a S/N of 3 was approximately 30 microg mL(-1) for either analyte. The method was used for the assay of MA or SO in pharmaceutical infusion solutions. The RSD values were 0.15% or 1.07% (n=6) when determining 100 mg mL(-1) of MA or 50 mg mL(-1) of SO in commercial infusion solutions. The results were in good agreement with those of pharmacopoeial iodimetric titration.
Subject(s)
Boric Acids/chemistry , Electrophoresis, Capillary/methods , Mannitol/analysis , Sorbitol/analysis , Electrophoresis, Capillary/instrumentation , Hydrogen-Ion Concentration , Infusions, Intravenous , Reference Standards , Reproducibility of Results , SolutionsABSTRACT
Eight phenolic acids were analyzed by capillary zone electrophoresis. On-line analyte preconcentration was carried out by hydrodynamic injection of large volume of sample followed by removal of the bulk of the low conductivity sample matrix by polarity switching. The optimal electrolyte system consisted of 50mM sodium tetraborate of pH 9.0 (adjusted with 0.1 M phosphoric acid) containing 2% of alpha-cyclodextrin. The separations were carried out with a fused silica capillary (effective length 50 cm, i.d. 50 microm) and monitored at 200 nm. Under optimized preconcentration conditions (sample injection 99 s at 100 mbar and the polarity switching time 1.0 min) linear calibration ranges (0.1-2.0 microg/ml, R=0.9979-0.9995), favourable limits of detection (0.01-0.025 microg/ml) and good repeatability of the peak areas (R.S.D.: 2.76-5.69%, n=6) were achieved.
